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Preparation method for optical transparent ordered inter-aperture silica single block

A mesoporous silicon oxide, optically transparent technology, applied in the directions of silicon oxide, silicon dioxide, chemical instruments and methods, etc., can solve the problems of high cost, difficult industrial production, long processing time, etc., achieve low cost, reduce drying and cracking , the effect of short production cycle

Inactive Publication Date: 2006-11-08
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods either require special equipment or reagents, or the processing time is too long and the cost is high, which has caused great difficulties in its industrial production in batches.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 2.0g of Brij56 in 4.0g of TMOS, stir vigorously in a water bath at 40°C, add 2.0g of HCl (pH=1.0) dropwise, wait until the solution is mixed into a homogeneous phase, continue stirring for 10 minutes, and then vacuum for 5 minutes. Put the sol into a hydrothermal kettle, seal it with a plastic wrap, and let it stand in a constant temperature drying oven at 40°C for 24 hours to gel and age. Inject 10.0mL of 1M HCl, seal the hydrothermal kettle tightly, and after hydrothermal treatment at 80°C for 72 hours, the gel will be released naturally and has good mechanical strength. Brij56 in the gel can be completely removed by extraction with 30 mL of isopropanol for 16 h. Finally, the gel was quasi-sealed in a beaker with a microporous plastic wrap, and dried at a temperature of 40-110° C. to obtain an ordered mesoporous silicon oxide monolith with a size of Φ30.0×3.0 mm.

Embodiment 2

[0020] Dissolve 3.2g of Brij56 in 8.0g of TMOS, stir vigorously in a water bath at 40°C, add 4.0g of HCl (pH=2.0) dropwise, wait until the solution is mixed into a homogeneous phase, continue stirring for 10 minutes, and then vacuum for 10 minutes. Put the sol into a hydrothermal kettle, seal it with a plastic wrap, and let it stand in a constant temperature drying oven at 40°C for 24 hours to gel and age. Inject 10.0mL of 1M HCl, seal the hydrothermal kettle tightly, and after hydrothermal treatment at 80°C for 72 hours, the gel will be released naturally and has good mechanical strength. Brij56 in the gel can be completely removed by extraction with 60 mL of isopropanol for 24 hours. Finally, the gel was quasi-sealed in a beaker with a microporous plastic wrap, and dried at a temperature of 40-110° C. to obtain an ordered mesoporous silicon oxide monolith with a size of Φ30.0×6.0 mm.

[0021] Example 2:

[0022] Dissolve 2.8g of Brij56 in 4.0g of TMOS, stir vigorously in a...

Embodiment 4

[0024] Mix 2.0g Tween40 and 4.0g TMOS, stir vigorously in a water bath at 40°C, add 2.0g HCl (pH=2.0) dropwise, wait until the solution is mixed into a homogeneous phase, continue stirring for 10 minutes, and then vacuumize for 15 minutes. Put the sol into a hydrothermal kettle, seal it with a plastic wrap, and let it stand in a constant temperature drying oven at 40°C for 24 hours to gel and age. Inject 10.0mL of 1M HCl, seal the hydrothermal kettle tightly, and after hydrothermal treatment at 100°C for 48 hours, the gel will be released naturally and has good mechanical strength. Extract with isopropanol for 16 hours to completely remove Tween40 in the gel. Finally, the gel was quasi-sealed in a beaker with a microporous plastic wrap, and dried at a temperature of 40-110° C. to obtain an ordered mesoporous silicon oxide monolith with a size of Φ30.0×3.0 mm.

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Abstract

The invention relates to a method for preparing an ordered mesoporous silicon oxide monolith. A method for preparing an optically transparent ordered mesoporous silicon oxide monolith is characterized in that the steps are as follows: 1) selecting materials: by mass ratio: nonionic surfactant: hydrochloric acid: methyl orthosilicate = 0.5~ 2:1:1~4, wherein the pH of hydrochloric acid=0.5~2; 2) Mix non-ionic surfactant, methyl orthosilicate, and hydrochloric acid solution and stir evenly; 3) Vacuum for 5~20 minutes to obtain A sol with lyotropic liquid crystal characteristics; 4) After the sol is gelled in a hydrothermal kettle, the gel is hydrothermally treated with deionized water or acid, alkali or salt solution at 60-120°C for 12-72h, and then washed with ethanol or isotropic Propanol is used as an extractant to extract and remove the surfactant; 5) Finally, after heating and drying at 40-110° C. for 10-48 hours, an optically transparent ordered mesoporous silicon oxide monolith is obtained. The invention has short processing period, simple procedure, good repeatability and does not require special equipment. The prepared mesoporous silica monolith is expected to be used in the fields of catalysis, separation, and especially optical functional materials.

Description

technical field [0001] The invention belongs to the technical field of chemistry and inorganic materials, and in particular relates to a preparation method of an ordered mesoporous silicon oxide monolith. Background technique [0002] Functional mesoporous composites loaded with specific functional molecules or nano-ion clusters show attractive application prospects, and a lot of research has been carried out in energy storage, nonlinear optics, low dielectric constant, chemical sensing, etc., especially nonlinear Optical composite materials require optically uniform and transparent amorphous ordered mesoporous monolithic matrix materials. In addition, because the traditional zeolite molecular sieve has a pore size in the micropore range (<2nm), large-sized molecules cannot enter. Under the background of the simultaneous depletion of petroleum resources, it has always been necessary to find a catalyst carrier suitable for the heavy oil catalytic industry to synthesize mol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18B01J21/08
Inventor 雷家珩刘丹郭丽萍赵俊巫辉
Owner WUHAN UNIV OF TECH
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